Oddy Test Protocols

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Disclaimer

Oddy testing information and protocols are provided for informational purposes only. Neither AIC nor participating institutions endorse particular methods, products, businesses, or services. The following protocols are not vetted or peer-reviewed and should be assessed by each individual user for the accuracy of the results.

To Contribute a New Protocol

Please follow the guidlines provided on the Discussion Page of this Page. Click the Discussion link at the top of the page. We are now providing a recommended list of sections for our protocol for ease of use in comparison between the protocols.

General Test Information

General test information can be found here.
A comprehensive bibliography of articles on the Oddy Test can be found here.

National Archives of Australia (NAA) PAT Protocol

The NAA carries out the Photographic Activity Test (PAT) according to the ISO 18916:2007 Imaging materials – Processed imaging materials – Photographic activity test for enclosure materials. The test is described on their site along with results of materials that have passed since 1996. The complete protocol is described in greater detail on the IPI site.

Getty Conservation Institute (GCI) Protocol by Mara Schiro

I. Experimental Overview

The principle of the Oddy test is that a sample of proposed storage or display material (the test material) is enclosed in an airtight reaction vessel with three small metal coupons: copper, silver and lead. This is a test of reactivity of gasses that evolve off of the test material, not a contact test so the metal coupons do not touch the test material or each other. The evolution of gases from the material and any corrosion reactions are accelerated by elevating the temperature to 60°C and adding a small amount of water to maintain the relative humidity at 100% for the duration of the test. For every set of samples, one control test is simultaneously carried out with water and the metal coupons but no test material to measure the effects of elevated temperature and relative humidity alone. These coupons in the control environment are called the blanks. After 28 days at elevated temperature and relative humidity, the experimenter visually assesses the degree of corrosion on the test coupons and compares them to the corrosion on the blank coupons. If no alteration has occurred to the test coupons, the material passes. If any corrosion has occurred on any of the coupons, the luminosity of one or more of the coupons has deteriorated or the color of any of the coupons has changed dramatically, the test material fails the Oddy test and the material is not recommended for use. The purpose of this test is not to identify what type of volatile compound is being released from the test material. A failure in the silver coupon could be an indication of the following types of gasses evolving off of the test material: reduced sulfur compounds and carbonyl sulfides. A failure in the copper coupon could be an indication of the following types of gasses evolving off of the test material: chlorides, oxides, and sulfur compounds. A failure in the lead coupon could be an indication of the following types of gasses evolving off of the test material: organic acids, aldehydes, and acidic gases. This list is not comprehensive and should only be used as a starting point for future research if more investigation is required.

II. Materials Coupon size does not effect corrosion but standard sizes are used for consistency of analysis. 1. New or used silver coupons (1 per sample + 1 for control) 1.1. Purity: metal foil of no less than 99.5% purity 1.2. Size: 10 x 15 mm by about 0.1 mm thick Goodfellow Silver foil AG000450/11 2. New or used copper coupons (1 per sample + 1 for control) 2.1. Purity: metal foil of no less than 99.5% purity 2.2. Size: 10 x 15 mm by about 0.1 mm thick Alfa Aesar copper foil 99.9%, 0.254mm thick, Stock #13379 3. New lead coupons (1 per sample + 1 for control) 3.1. Purity: metal foil of no less than 99.5% purity 3.2. Size: 10 x 15 mm by about 0.1 mm thick Alfa Aesar lead foil 99.9%, 0.1mm thick, Stock #42708 4. Felt-tipped rotating polisher Freedom Electric Company, Serial # C850026 5. Metal polish: polish metal fledge metal-polish from SPI supplies, Stock #1027 6. Lint-free polishing cloth 7. Mr. Clean liquid cleaning solution 8. Toothbrush or other soft-bristled brush for cleaning 9. Acetone 10. Deionized or distilled water 11. Small well-sealed clean glass jars VWR, I-Chem brand 60 mL jars (P/N 15900-242) 12. Glass ring no more than 3cm in diameter, or beaker of same size (20mL) 13. Glass test tubes VWR, Disposable Culture Tubes (P/N 47729-566), Durex Borosilicate Glass Size 6x50 mm 14. Clean single-use gloves (2 pairs) VWR, Esteem Stretch Nitrile Gloves (P/N 8817N) 15. Safety glasses 16. Clean tweezers 17. Kimwipes or other lint free laboratory-grade tissue paper

III. Sample Selection

1. The sample should be freshly obtained from the manufacture. • Most materials are most corrosive when first produced and should be tested in this state. • Manufacturers can change formulation of their products at any time without notification so you cannot test an old material if new material will be used. 2. In the case of composite materials (i.e. epoxies) the sample should contain all components in the form that they will be used. 3. Paints, varnishes and adhesives should be tested as freshly cast films. 4. Each sample should be approx. 1x1x1 cm in size to easily fit into reaction vessel. 5. Approximately 2 grams of test materials should be used. With lighter bulkier materials is may be impossible to use that much sample and the following guidelines can be used instead: • Dense materials (i.e. epoxy) at least two 1x1x1 cm cubes • Bulky materials (i.e. foams and boards) four to six 1x1x1 cm cubes • Light materials (i.e. fabrics or paints) ten to twenty 1x1 cm squares

IV. Coupon Preparation

You will need one of each coupon per sample plus one extra of each coupon for the control. For those inexperienced with the Oddy test, consider preparing 2-5 replicates of each sample and of the control to ensure accurate results and prevent false-negatives.

1. Polish Coupons 1.1. Put on clean gloves and safety glasses. 1.2. Cut new lead coupons using clean scissors and set aside until Reaction Vessel Set-Up. • DO NOT polish or wash lead coupons. 1.3. Select new or used silver coupons to polish. 1.4. Select new or used copper coupons to polish. 1.5. Use metal polish and felt-tipped rotating polisher to remove corrosion and tarnish from the front, back and sides of each coupon so that they are untarnished and shiny. • Always wear safety glasses and gloves when polishing. • Polish all silver and copper coupons even if they are new. 1.6. Use lint-free cloth to finish polishing and remove all residue, making sure to thoroughly clean front, back and sides of each coupon. • From this point forward, only handle coupons with tweezers!

2. Clean Coupons 2.1. Put on clean gloves. 2.2. Submerge silver and copper coupons in Mr. Clean liquid cleaning solution. • Mr. Clean is used because (unlike dish soap or detergents) it doesn’t leave a residue. • DO NOT polish or wash lead coupons. 2.3. Remove one coupon at a time from cleaning solution using tweezers and scrub both sides with a toothbrush against the palm of your gloved hand. 2.4. Thoroughly rinse each copper or silver coupon with dionized or distilled water. 2.5. Submerge coupons in acetone. They can either be removed immediately or left submerged for short periods of time while remaining coupons are cleaned. 2.6. Using tweezers, remove coupons from acetone a dry with a kimwipe. 2.7. Using tweezers, carefully inspect all coupons to ensure they are free from tarnish, residue, corrosion, dust or finger prints.


V. Reaction Vessel Set-Up You will need one reaction vessel per sample plus one extra for the control. 1. Thoroughly clean reaction vessel (I-Chem brand 60mL jar) using Mr. Clean. 2. Rinsing three times with deionized/distilled water and dry with a lint free cloth. 3. Label reaction vessel with a unique sample ID number (instructions below in VII. Using Computer Database VII.22. VII. .2Obtain a new sample ID) 4. With gloved hands, bend each coupons over the glass ring or beaker so that the coupons are suspended in an upside-down U or V shape and don’t touch one another. 5. Gently place ring into jar. 6. Arrange test material samples inside or around outside of ring ensuring that none of the sample is in contact with the coupons. 7. Fill two test tubes with water. If your material is perticuarly absorbent, you may need to fill more than 2 tubes to maintain 100% relative humidity throughout the duration of the test. • The ideal water to air volume ratio of 1:100 8. Check that none of the coupons touch the test material or each other. 9. Tightly seal jars. 10. Place in 60° oven. 11. After a half hour in the oven, re-tighten the jars and return to the oven.

VI. Analysis of Results

1. After 4 weeks (28 days) remove reaction vessels from oven.

2. Open each reaction vessel and using tweezers to remove metal coupons and lay them out onto a labeled piece of paper.

Control Blank Test Material Sample ID Test Material Sample ID Silver (Ag) Copper (Cu) Lead (Pb)

3. Discard test material in trash and discard glass test tubes in glass disposal container.

4. Classify the results for each metal coupon as follows: • P = Permanent. No visible corrosion. Suitable for permanent use. Coupons should not have lost luster on polished surfaces. All copper coupons including the control will naturally turn a darker orange when exposed to heat and humidity. Some lead coupons including the control may acquire a slight purple hue. • T = Temporary. Slight tarnish or film of corrosion, discoloration. In the guidelines for the test these are considered suitable for temporary use. However, the Getty practices a more conservative approach and almost never uses materials that have been deemed suitable for temporary use. • U = Unusable. Corrosion clearly visible. Unsuitable for display case or storage use.

Cleveland Museum of Art (CMA) Protocol


Test Method Description:
Testing methods were adapted from the Philadelphia Museum of Art. For all testing, the oven is set to 35 degrees Celsius. Samples are prepared with clean tools to avoid contamination. Nitrile gloves are worn during sample and coupon preparation and changed between polishing compounds. Information is recorded and collected on spreadsheet and since 2012, photos are taken of the coupons after the test is finished.
Starting in 2014, the sodium azide test has been used to eliminate fabrics prior to Oddy Testing.

Sample and Beaker Preparation

Fabric pouch.jpg


1. If tested material is fabric, wash in two rinses of cold tap water to duplicate industrial washing process of fabrics used in exhibition cases.
2. Prepare one 1000 mL Pyrex beaker and one 16 oz Pyrex jar for each material tested plus an additional beaker and jar for the batch control. Rinse each piece of glassware with deionized water followed by wiping with acetone on cotton pads. Cover with aluminum foil until needed.
3. For each fabric tested, sew five cloth bags.
4. Roll a sheet of aluminum lengthwise to form a 1/4 inch rod and place over top of beaker, crimping edges to secure. Repeat for each piece of glassware used in testing.
5. Fabric bags can be tied to the aluminum rods with Nylon monofilament or cotton thread used for making bags. Other types of materials tested can be balanced on an upside down jar or beaker placed in the bottom of the outer beaker. Tested materials do not touch the water. If fabric gets wet due to excessive condensation they are redone.
6. Cover each beaker with two pieces of aluminum foil and crimp loosely. Inscribe the associated sample number into the aluminum foil with a bamboo skewer.

Note: Coupon preparation is done on a clean, disposable work surface to prevent contamination. Scissors or scalpel are cleaned between cutting each type of metal. Individual coupons are cut after polishing is complete.

Preparing Silver (Ag) and Copper (Cu) Coupons
1. Fill ultrasonic cleaner with deionized water and turn on for five minutes to allow degassing.
2. Calculate total size of metal foil needed for testing: two 1 x 0.25 inch coupons of Cu and Ag are required for each material tested. One for "accelerated" test container in the oven and one for "ambient" test container at room temperature.
(2)(0.25) x (# of tests + 1 control) = total size of foil in inches
3. Degrease each foil sheet by swabbing or soaking for one minute in naphtha, then ethanol, and finally acetone.
4. Wearing clean gloves, rinse three times in acetone and dry with clean cotton pad or kimwipe.
5. Coupons are not reused, so do not require corrosion removal or much polishing.
6. Polish foils with 1 μm alumina and rinse with deionized water. Examine under microscope to check for corrosion. Repeat until surface is clean.
7. Immerse metal foil in ultrasonic cleaner for 23-30 seconds.
8. Rinse with acetone and air dry. Examine under microscope to check for polish residue. Repeat rinsing until clean.
9. Cut foil into individual coupons with clean scissors.

Preparing Lead (Pb) Coupons
1. Calculate total size of metal foil needed for testing: one 1 x 0.25 inch coupons of Pb is required for each material tested.
(0.25) x (# of tests + 1 control) = total size of foil in inches.
2. Degrease foil by swabbing or soaking for one minute in acetone and xylene.
3. Wearing clean gloves, rinse three times in acetone and dry with clean cotton pad or kimwipe.
4. Coupons are not reused, so do not require corrosion removal or much polishing. Remove corrosion or surface discoloration with smallest grit size of abrasive paper that works efficiently (220 or 600). Examine under microscope to check for corrosion. Repeat until surface is clean.
5. Rinse three times in acetone and rub dry. The metal may darken slightly at this point.
6. Examine under microscope to check for polish residue. Repeat rinsing until clean.
7. Cut foil into individual coupons with clean scissors.

Completing the Setup

Fabric test in beaker.jpg

1. Each accelerated test jar receives one silver and one copper coupon. Each ambient test jar receives one silver, one copper and one lead coupon. Use clean plastic tweezers to place coupons in appropriate fabric bags or on top of sample material. The goal is to have each coupon half in contact with the sample and half not in contact with anything. Coupons can be bent if necessary. The control coupons are usually pierced and tied to the aluminum rod with monofilament or cotton thread. Replace aluminum lids on jars.
2. Accelerated test beakers: Pour 50 mL deionized water into bottom of 1000 mL beakers. Cover with 2 layers of aluminum foil and place in the oven.
Ambient test jars: Pour 25 mL deionized water in bottom of each 16 oz jar. Cover with aluminum foil so 1 inch of the side is covered and cut off excess. Wrap Teflon tape around edge of foil to create air seal. Store at 21 degrees C.
3. Check coupons for corrosion under the microscope after 28 days and compared to the control coupons. Coupons may be checked earlier to eliminate non-usable fabrics.

Time Period Method Used: 2009-current

Autry Museum Protocols by Ozge Gencay Ustun


We have adopted and adapted Brooklyn Museum's Oddy Test procedures according to our needs and experience with the test.

I. Materials you will need:

  • 45 ml glass Kimax weighing bottles with gorund glass outside caps
  • 20 ml beakers
  • Metal coupons, silver, copper, and lead (do not reuse lead or copper coupons, this may result in inconsistent results)
  • Deionized water
  • Cotton swabs
  • Acetone in a jar (use a separate jar for lead coupon cleaning)
  • High vacuum silicone grease (Dow Corning)
  • 2 glass bristle brushes (one for silver one for copper, don't polish lead to reduce health hazard)
  • Gloves
  • pH-indicator strips
  • pliers or scissors for cutting coupons
  • Disposable plastic 1ml transfer pipette
  • Lab glassware cleaning detergent
  • Glass wool (optional) (see procedure 9 below)


II. Test Preparation:


1. As you work, fill out the Oddy testing form. Be sure to include as much information as possible. If necessary attach a sample of the material to the form.
2. Use clean glassware. The glassware should have already been thoroughly cleaned with any lab glassware cleaning detergent and rinsed with deionized water. Rinse glassware several times with deionized water again just before use.
3. Put on gloves. For the rest of the test, nothing can be contaminated with bare hands. You must wear gloves at all times.
4. Using cotton swabs, wipe the glass containers, glass beakers and small vials with acetone. Set these pieces aside to air dry completely. Any residual solvent could contaminate the test.
5. Label your jars with the number corresponding the test material on the form.
6. Next, clean the metal coupons with a glass bristle brush. Work on a clean surface such as a piece of Mylar. Change the Mylar with each new coupon so they are not contaminated. There is a separate brush for each of the metals. Again, do not touch the coupons with bare hands. After cleaning with brush, dunk the coupons in their appropriate jars containing acetone to wash them. Take them out after a couple of minutes and let them air dry. Set aside. Handle lead with gloves and don’t polish them.
7. Weigh the material (it should be around 1.000 gr and/or fit in the 20 ml beaker) and place it in the beaker first.
8. Then insert the coupons (unbent) between the material and the beaker. Half of the coupons should touch the test material and half of it should not touch the material. This way one can test the direct impact of materials with contact and indirect impact of off-gassing when there is no contact of the material with the coupon. There will always be a setup that will be used as a control with no sample. In order to insert the coupons in the control beaker use glass wool wad (inert material) or the coupons can be bent and hang on the lip of the beaker. Do not let the coupons touch each other.
9. Pipette 1 ml of deionized water into the kimax jar.
10. Carefully place the beaker (with sample and coupons) into the Kimax glass weighing bottle. Use tweezers to lower it in.
11. Run a light amount of grease along inside the lid of the Kimax ground glass fitting with the Dow Corning high vacuum grease. Place the lid on the container lightly, rotate the lid to distribute the grease evenly and then press down tight to form a good seal. Be careful not to disrupt your coupons or the water filled glass vial. The coupons should not touch each other. Do not press hard on the lid or wiggle the lid to close it tight in the jar. This may later cause freezing of the ground glass joint after the test.
12. Place jars in lab oven. The temperature should be 60˚ C (~140˚ F).
13. Check the jars periodically (once a week) to make sure the water has not evaporated. Water evaporation indicates potential loss of VOC’s from the container – nullifying test. Avoid moving the containers to keep any water droplets on the lid from dropping onto the coupons.
14. After 28 days, remove the jars and immediately open the lids as you remove them from the oven (otherwise the lids may freeze shut forever). Record the results on the Oddy testing sheet. Ask another conservator to look at the coupons in your absence and w/o knowing your results or the materials. Compare the degree of corrosion on the metal samples to the control. Recommend whether the material fails completely, passes for temporary exhibition (~3 months), or passes for long-term use and write this on the sheet. Mention whether materials touching the coupons corroded more, less or similar when not touching the coupons (only the fumes are exposed). This way one can also recommend to use a material but with restrictions or no restrictions of contact of the material with artifacts.
15. Write a memo with your results to the departments requesting the test.
16. When your test is finished, clean your glassware. Wipe off excess vacuum grease with a paper towel first, and soak/clean in detergent tub separate from all other lab glassware. Once clean, rinse with deionized water. Once dry, place glassware back into Oddy testing tub.
III. Containers:
We have switched from the glass jars with I-Chem blue polypropylene lids for a couple of reasons. It was not possible to consistently obtain a good seal resulting in loss of moisture and VOC’s from the test material, which nullifies the test. In addition the polypropylene lids didn't last long in the oven at 60 degrees C. The test is dependant on a consistent 100% RH environment. With oven heat, the plastic lids expanded, softened and eventually developed cracks.
IV. Water:
The amount of water is dependant on the volume of the container. The ratio is roughly 1:100 water to container volume. The volume of the Kimax weighing bottle with cap is roughly 65ml, so 0.6ml of water should be added to the vial in the container. We have had better condensation results with 1 ml water (while still providing 100% RH), so 1 ml is recommended. Excess moisture will often result in corrosion of the lead coupon, providing a false result. Large droplets of water on the lid of your container dripping on the coupons or test material indicates excess water. This is less likely to occur if your test material absorbs moisture (wood or paper materials), and morelikely to occur with non-absorbing materials.
V. Materials:
Kimax Weighing Bottles with Ground Glass Outside Caps. 45 ml, 40 x 50 mm, 45/12 #03-422F ($182/6 pack; $30 each, can be found on eBay) Kimax Griffin Beakers. 20 ml #02-539-1 ($74.45/12 pack) Dow Corning High Vacuum Grease. 5.3 ox tube #14-635-5D ($25) All from Fisher Scientific (800) 926-1166

Copper foil (Cu000690) (as of June 2009) Thickness 0.3mm 300x300mm 99.98% Half hard temper flattened (GoodFellow Limited) Lead Foil. Pb0004000 Thickness 0.5 mm, 500x500mm, Purity: 99.98% PB0004000/23 (GoodFellow Limited) Silver foil 0.005" thick 99.98% purity (Sigma Aldrich Chemical Company)

Industrial Fine Eraser (metal body fine Fyberglass eraser) #AA2120 E113/F (The Eraser Company Inc. (315) 454-3237) Replacement for glass brushes (24 pack) ([glassradierer-ersatzpinsel]]) Dow Corning High Vacuum Grease 5.3 oz tube #14-635-5D (Fisher Scientific) ph-indicator strips P4786 Sigma Aldrich

British Museum Protocols


Oddy tests are performed using the ‘3-in-1’ version of the test as described in the publication Selection of materials for the Storage or Display of Museum Objects. For dry or bulk samples such as paper, fabric, boards etc., a 2 g sample is used wherever possible. Unless otherwise specified, paints are spread onto a piece of Melinex (polyester film) and allowed to air dry for four weeks, with a 12 cm x 6 cm sample size used for each test. The preparation of other sample types such as adhesives is currently under review.
pH tests are carried out for fabrics and papers. A pH test is carried out to help predict whether the material tested can safely be placed in direct contact with an organic object. The pH should be between 5.5 and 9 if the tested material is to be in direct contact with organic materials. When the pH test is performed, it is also possible to assess whether the tested material is colourfast. If the material is not colourfast, it is advised that it is not used.

Interpreting results in the Database of Materials Test Results
Oddy test results: Test results are recorded for each individual metal used in the test. However, an overall rating is assigned to indicate a material’s general suitability.

pH test results: A material with a fugitive (non-colourfast) dye or a pH value outside 5.5-9 will be classified as an unsuitable material.

The overall rating for the material is shown results table and is determined by the worst test result obtained. Pass- Suitable for permanent use; Temporary- Suitable for temporary use (less than six months); Fail- Unsuitable, do not use.


The data published in the Database of Materials Test Results (‘the database’) is regularly updated and revised. It contains the results of research work carried out by the British Museum within five years of the most recent update.

The British Museum does not use or rely on any version of the database, or any data contained within it, which is more than five years old. In making any predicative assessment of the suitability of materials based on the Oddy test or the pH test, the most up to date version of the database published on the British Museum website is the only current and authoritative statement of British Museum opinion at any given time.

The Green Challenge Protocol by Christian Hernandez


This protocol was heavily inspired by “Testing Materials for the Storage and Display of Artefacts” by Thickett and Green, and developed for the 2012 graduate thesis work of Christian Hernandez.

I. Supplies:

  • Oven: A Blue M Stabil-Therm® Bench Type Gravity Convection Laboratory Oven Model OV-12A was used by the tester
  • Metal Foils at >99.5% purity: Lead, Copper, Silver
  • Glass Test Tubes: 3-50 mL + 3-1 mL vials per material + Control
  • Silicon Stoppers for each 50mL test tube.
  • Distilled Water: .5 mL / 1 mL vial. pH 7. pH strips, NaOH
  • Clean Surfaces: Cover surfaces with Mylar/Paper.
  • Equipment: Camera, Stereomicroscope, Scale
  • Documentation: Temperature log, Materials Log
  • Glass Bristle Brushes: 3. Label with what metal it is used with.
  • Materials to be tested: 6 gm/material + sample
  • Test Tube Tray(s)
  • Piece(s) Coroplast: Tray-Sized, Velcro
  • Acetone/Alconox
  • Kim-Wipes/Cotton Swabs
  • 2 Tweezers
  • Box of Powderless Nitrile Gloves
  • Small Transfer Pipette/Dropper
  • N-19 respirator
  • Scissors, Xacto-knife
  • Teflon Tape


II. Protocol
Before beginning, select your materials and keep a sample for future reference. Record the material's name, retail product ID#, Manufacturer and/or retailer, date purchased and notes (finishes, colors etc.). Assign each material an ID#, with the first number for the control and the second for the material. A table like the one below may be helpful in keeping track of this information.

ID# Name Product ID Manufacturer/Retailer Date Purchased Notes re: finishes, colors etc
1 Control NA NA NA NA
2 Ethafoam® HRC® DNA Manufactured and sample from Sealed Air Sample Received Feb 2012 Black, 2" thick
3

Day 1: Preparing Equipment
Note: Document all stages with photography. Wear gloves at all times.

  1. Gather all materials needed in advance. Make sure the distilled water is pH 7. Use NaOH if needed.
  2. Label test tubes with the metal and material ID. Create a system for placement on trays if need be.
  3. Treat all testing materials in the state they may be used (wash textiles, boards don’t need anything etc).
  4. Wash the test tubes in warm water and then rinse in distilled water.
  5. Preheat oven to 60 oC.
  6. Set prep areas (see below for materials needed).


Day 2: Preparing Materials & Beginning Test

1. Processing Testing Materials
Note: This can be done the day before if left undisturbed
Materials needed: acetone, Kimwipes, scale, scissors/Xacto knife, materials to be tested

  1. Wipe tools before and between materials.
  2. Using a scale, measure out 3 – 2 gram amounts of materials to be tested (one for each metal).
  3. Cut or delaminate each sample amount into small pieces to increase surface area exposed during test.
  4. Store each sample in a sanitized location (a new polyethylene bag, or beaker, etc).


2. Test Tube Preparation
Materials needed: acetone, Kimwipes, tweezers, test tubes, vials, silicon stoppers, Xacto knife, pipette/dropper, distilled water

  1. Wipe tools before and between materials.
  2. Wipe test tubes, vials and silicon stoppers with acetone using a Kimwipe, tweezers.
  3. Rinse inside of test tubes with acetone.
  4. Place 2 g of materials to be tested into bottom of test tube.
  5. Using a pipette/dropper/syringe, place .5 mL of distilled water in vial.
  6. Gently lower vial into test tube making sure not to spill any water.
  7. Cut a slit into silicon underside of stopper using Xacto knife (this is where the coupon will go).


3. Coupon Cleaning and Completing Test Preparation
Materials needed: acetone, Kimwipes, tweezers, Mylar, glass-bristle brushes, metal foils, scissors, gloves

  1. Wipe tools before and between materials. Use new gloves with each material and then dispose after.
  2. Set three stations with clean Mylar for surface and correct glass-bristle brush.
  3. Cut metals into .5 cm x 1 cm coupons (specific weight?).
  4. Polish and degrease each coupon with glass bristle brushes. Wear respirator mask when working with lead.
  5. Wipe coupon with acetone and Kimwipe.
  6. Coupons must not touch each other or any other surface. Immediately put coupons in slit in silicon stoppers as vertical as possible to reduce condensation from forming on the coupon.
  7. Place corresponding silicon stopper with marked test tube (copper with copper etc).
  8. Seal test tube with thread-seal tape.
  9. Place Coroplast over filled test tube tray and.
  10. Place filled test tube trays in oven and close door.


Day 3-31: In the oven
For the following 28 days, the oven should be monitored and a daily log kept with the temperature noted. If the temperature fluctuates drastically then the test may be corrupted. A table like the one below was used to record this information.

Day - Date Time Temperature/observations Observer
1 - dd/mm/yyyy 00:00 PM xx°C CH
2 -
3 -


Day 31 – Gathering the results
Materials needed: clean work area, camera, tweezers,

  1. Turn oven off and carefully open door. Note if any test tubes have broken or popped (rare).
  2. Carefully remove test tube tray (may need piece of handling cloth, gloves) and place on work surface.
  3. Keeping the test tubes vertical, inspect the materials for degradation and note observations.
  4. Keeping the test tubes vertical remove the thread seal tape and the silicon stopper with the coupon inside.
  5. Remove the coupon stopper, record observations and repeat for all test tubes.
  6. Assign a result (P, TP, U) and record on following page along with the attached coupons. (Note: The test is corrupted if the control has corrosion.)
    P - Pass: suitable for long-term use; no change compared with control. Red/orange iridescence may appear on the copper control. Coupon should not have lost polished surface. Lead control coupon may acquire a purple hue. Aqueous corrosion has occurred on lead control coupon on a few occasions.)
    TP - Temporary Pass: suitable for indirect short term use; slight/questionable discoloration only, often seen along lower edge and sides or as a few localized small spots.
    U - Unsuitable for use: clearly visible corrosion or loss of polish, thin layer of corrosion over surface
  7. Photograph or scan both sides of the coupon and make sure to keep a log of photos as to not get them confused. The physical coupons may continue to corrode so these images will be the best visual record of the test results. Keep the coupons in a table such as the one below.


ID#, Material Coper Lead Silver Result (P, TP, F)
1. Control (physical coupon) (physical coupon) (physical coupon) (Result)
2. Ethafoam® HRC®
3.

Silver Nanofilm Sensor Protocol to test housing materials for Daguerreotypes by Robyn Hodgkins et. al.



The following protocol is outlined in the following article "Silver Nanofilm Sensors for Assessing Daguerreotype Housing Materials in an Oddy Test Setup" published by Robyn E. Hodgkins, Silvia A. Centeno, Joseph A. Bamberger, Masahiko Tsukada, Alejandro Schrott in e-Preservation Science, 2013. In this work, an Oddy test enhanced with silver nanofilms was utilized for evaluating a variety of materials typically employed for housing sensitive silver images, including daguerreotypes. The silver nanofilm sensitivity was compared to silver foil used in the standard Oddy test and to daguerreotype image samples. The resulting procedure allowed for facile visual evaluation of the silver films after exposure and reduced the length of the test.


Experimental Materials:
The Oddy test materials include:

  • silver foil (Aldrich, 0.025 mm, 99.9%),
  • copper foil (Aldrich, 0.127 mm, 99+%),
  • lead foil (Alfa Aesar, 0.1 mm, 99.9%),
  • 20 mL Pyrex beaker (Corning Incorporated),
  • 125 mL I-Chem clear short wide mouthed jar and lid (Fisher Scientific),
  • Dow Corning high vacuum grease, and
  • deionized water.


Silver film materials include:

  • silver shots (Aldrich, 1-3 mm, 99.99%) and
  • petrographic slides (Buehler, 27 x 46 mm).


Slide cleaning supplies include:

  • Alconox (anionic powder detergent, Alconox, Inc),
  • ethanol (HPLC grade, Fisher Scientific),
  • acetone (HPLC grade, Fisher Scientific),
  • hydrochloric acid (ACS Plus, Fisher Scientific),
  • crystallizing dish (170 mm, Pyrex),
  • shaker (Thermolyne Rotomix Type 48200), and
  • Dust Off dis- posable compressed gas duster.



The gilded daguerreotype samples used in this study, made by contemporary artist Jerry Spagnoli, were examined by SEM-EDS before testing and were found to have image particles within the typical range of diameters and compositions of those observed in 19 th century plates.

Procedure

Before silver film formation, glass slides were cleaned in a crystallizing dish to remove surface contaminants as follows: 1) washed for 15-30 min in an aqueous solution of Alconox; 2) rinsed briefly in deionized water to remove residual Alconox; 3) washed in 1% v/v HCl for 15-30 min to remove any residues; 4) rinsed in deionized water and washed for 15-30 min in water to remove HCl; 5) rinsed briefly in ethanol then washed in ethanol for 15-30 min to dehydrate; and 6) rinsed and washed with acetone for 15-30 min to finish cleaning. After cleaning, slides were submerged and stored in acetone at room temperature until use. Slides were dried immediately before use with a compressed gas duster. Silver nanofilms were made using an Edwards Vacuum Coating unit E306A comprised of an E2M8 rotary vacuum pump, E04 vapor diffusion pump, Pirani 10 vacuum gauge, Penning 8 vacuum gauge, FTM6 quartz crystal microbalance film thickness monitor, and a variable transformer. The films were formed under a vacuum of 2 x10 -6 mbar at a deposition rate of 0.025 nm/s to a desired thickness of 7- 200 nm. The films were stored in a sealed bag with silica gel condi- tioned at 33% RH to prevent tarnishing when not immediately used.

Testing
The MMA 3-in-1 Oddy test configuration is described in detail by Bamberger et al. 8 For this method, deion- ized water (2 mL) is added to the I-Chem jar first. The metal foils are folded over the edges of the 20 mL beaker and the material to be tested (typically 2” x 1”) is placed inside the 20 mL beaker which is then secured with grease to the bottom of the I-Chem jar. The threads of the jar are coated with grease and the jar is sealed. The test setup is placed in the oven at 60 °C for 4 weeks. After the first 5 min in the oven, the lid is tightened another eighth to a quarter turn. A subset of materials was also tested using 1 mL of deionized water for comparison.

Oddy test using daguerreotype image sample, silver foil, and wool The standard Oddy test assembly was used for daguerreotype image sample tests. Only silver foil was used and the daguerreotype image sample was placed at the bottom of the beaker with the wool sample but not in contact. Tests were conducted for 1, 2, and 4 weeks at 60 °C.

Oddy test using silver nanofilms The Oddy test involving the silver nanofilms used the same glassware assembly as the 3-in-1 Oddy test. The material of interest was placed at the bottom of the 20 mL beaker and the silver nanofilm slide was placed on top of the sample (Fig. 1). The test setup was placed in the oven at 60 °C for 1 or 2 weeks.

Evaluation:

Rating of materials For the standard Oddy test, corrosion results were ranked on the scale from 1 to 5; 1 being no obvious change and 5 being obvious change in color with majority of the surface corroded. The ranking for all three metals are compared and a final overall rating is given for the material: pass (P), temporary (T), or unsuitable (U). 7,8 If a 4 or 5 ranking is given for one metal, the material is considered unsuitable. For the Oddy test with silver nanofilm, corrosion results are pass with no obvious discoloration, or unsuitable with brown discoloration that can be a few spots or the entire film. Daguerreotype image samples, nanofilms, and foils were photographed before and after each test using a Canon EOS 5D Mark II camera and Interfit Digilight 600 lights with Canon EOS Utility and Adobe Lightroom 3 software programs.

Cincinnati Art Museum (CAM) Protocol

There is no protocol information at this time.

Heritage Conservation Centre Singapore (HCC) Protocol

The Heritage Conservation Centre (HCC), Singapore, carries out the “3-in-1” Oddy test, adapted from published protocols used at the British Museum (BM occasional paper number 111 2004). The first protocol undertaken at the HCC between 2009 and 2016 used a heat shrink tubing and ground glass stopper with nylon monofilament (Thickett and Lee 1995) and silver, lead and copper coupons were separated with glass beads. Since 2017, the second protocol uses a silicon stopper with cut slots to separate the coupons (Robinet and Thickett 2003). According to needs and experiences, HCC adopts two notable variations from the British museum protocol, which are triplicate testing and glassware cleaning procedure. In triplicate testing, three tubes containing the same sample are tested and an overall pass is indicated for the sample if two or more tubes pass the test. In the glassware cleaning procedure, an additional step in evaluating the glassware suitability of use is employed.

Second protocol since 2017

Sample preparation The thumb of rule is to prepare the material as they are used in exhibition or storage.

  • For paints, adhesives and sealants, apply coating on a piece of cleaned Mylar and allow it to cure according to exhibition / storage use. After drying, scrape off 2 g of coating or roll the painted Mylar into the glass vessel.
  • For fabric, cut, roll and secure it with a cotton thread. Washed fabric: For organic fabric, the fabric is boiled repeatedly until water runs clears. For synthetic fabric, the fibres are washed at 60° C until water runs clear.
  • For foams, which are less dense, it may not be possible to squeeze 2 g into the tube. It is acceptable as long as the tube is sufficiently filled with the sample material, without touching the metal coupons.
  • For glass cleaning agents, use a paper towel immersed with cleaning agent to clean the interior of the glass vessel.


Glassware cleaning procedure

  • Fill glass tubes with cleaning solution of 2 % Decon 90 in deionised water and soak for 2 hours. Ensure no air bubble is trapped in glass tubes.
  • After soaking, rinse the glass tubes with deionised water several times to remove any soap.
  • Perform the ‘water test’. ‘Water test’ is carried out by overturning the deionised water filled tube. The glassware is considered clean when water flows smoothly down the glass surface, without water droplets clinging onto the glass surface within 10 sec.
  • For glassware that failed the water test, repeat soaking in 5 % Decon 90 for 2 hours. Then perform the ‘water test’ again. If persistent residue is left in glass tubes, ultrasonicate these glass tubes for about 6 min in 2 % Decon 90. If residues cannot be removed, avoid using the tube.
  • For those tubes that passed the ‘water test’, dry the glass tubes in the oven until use.


Preparation of coupons

  • Prepare metal coupons in a fume cupboard or extractor.
  • Wipe all metal trays and tools with acetone and cotton wool. A separate fibreglass bristle brush and metal tray is designated for each metal type to prevent cross-contamination.
  • Measure and cut out a metal sheet.
  • Place metal sheet over a glass block in its respective metal tray and use the respective fibreglass bristle to abrade one side of the metal sheet in two perpendicular directions.
  • Continue the abrasion until the surface of the metal appears evenly polished.
  • Turn the metal sheet to the other side and repeat the abrasion in two perpendicular directions.
  • When the abrasion is satisfactory, wipe the metal surface with a clean and dry cotton wool to remove remnant fibreglass and metal particles. If particles remain, clean the remnants with 99,9 % purity acetone.
  • Keep the metal coupons as flat as possible.
  • Clean all tools with acetone after use.
  • Using a scalpel, make three parallel slices at the bottom centre of the silicon stopper.
  • With one hand, pinch the silicon stopper to open the cut and insert the metal coupon with tweezers.
  • Start with inserting the lead coupon at the middle cut, followed by the silver and copper coupon at the auxiliary cuts.


Loading of samples

HCC Oddy Test Set Up
  • Add deionised water into the fusion tubes (mini-glass tubes) and close the opening with a small plug of cotton wool. The size and porosity of the cotton wool plug shall be as uniform as possible according to past practices. Ensure that the cotton wool plug is dry and not wet with water.
  • For highly absorbent materials like fabrics, add 0.6 ml deionised water. For low absorbent materials like paint, add 0.4 ml deionised water.
  • Place the sample, fusion tube and metal coupons assembly into the glass tubes.
  • Load three tubes without sample materials as negative controls.
  • Ensure that the sample is not in contact with the metal coupons. Ensure the metal coupons are flat. Ensure that the metal coupons are neither touching the inner walls of the boiling tube nor each other.
  • Leave the glass tubes in the oven at 60˚C for 28 days.


Metal coupon evaluation

  • When removing the “Oddy test vessels” from the oven, check that the temperature is at 60° C. Check for any condensation of water vapour in the tubes upon cooling and whether the coupons are freely suspended.
  • Remove the coupons from the tubes and place them on a white sheet of paper.
  • Rate the metal coupons with P (pass), T (temporary) or U (unusable) relative to the control coupons.
  • A pass is indicated if all coupons are rated P or T and a fail is indicated if any one coupon is rated U. Rate this for all triplicate tubes for each sample. Rate the sample pass if more than two tubes are rated pass.
  • Photo-document the results.



Auckland War Memorial Museum (AWMM) Protocol


Oddy test procedure:

Cleaning of glassware:

  • Glassware is cleaned with water and detergent.
  • Cleaned again with solvents if necessary
  • Rinsed with DDI (distilled, de-ionised water)
  • Flame cleaned by heating in a flame to drive of adsorbed water and other volatiles.


Coupons:

  • 99% pure or better preferred Pb, Cu and Ag.
  • Approximately .125 mm thickness preferred (0.005 inch)
  • Cut to 1cm x 3cm.
  • Remove surface oxidation/dirt with glass bristle brushes immediately before test.
Auckland Oddy Test Set Up
  • Rinse in acetone.
  • Insert in silicon stopper.


Set up:

  • High purity silicon stoppers, cut with 3 slices across the bottom
  • 1 of each coupon (Pb, Cu, Ag) placed in each slice.
  • 5ml glass sample tube filled with distilled water and stoppered with cotton wool place in the bottom of each test tube.
  • 1.0g-2.0g of sample place in the test tube and stopper inserted.
  • Duplicate runs of samples done if possible (usually only run one duplicate of the control).
  • Test tubes placed in an autoclave/oven at 50°C-60°C.
  • Visually inspected and notes taken at least once a week, for 4 -6 weeks (usually just 4 weeks).
  • Significant changes to the coupon surface compared to the controls recorded as a fail. Lead coupons usually become white/fuzzy/yellowish if they fail. Copper coupons may become black, brown, green, blue or other colours if they fail. Silver coupons usually darken/blacken if they fail. Pb Controls may become darker/paler, more matte, or slightly iridescent purple. Cu controls usually darken to a more orange/iridescent red colour, and may have darker spots from slight surface contaminants. Ag controls usually show no change, or slight spots of matte surface if contaminants are present.



Metropolitan Museum of Art (MMA) Protocol

Current Protocol:
Download and view this PDF for a full version of the MMA’s most current protocol: 20171116_OT.

Current photos of scored coupons from permanent, temporary, and unsuitable categories:
Copper Coupon Library
Silver Coupon Library
Lead Coupon Library

The Met’s previous version (20160416_OT), that incorporated silicone stoppers, is also available for download: 20160416_OT.
Minor Variations to protocols 20160416_OT & 20171116_OT (20160620_OT through 20180821_OT) can be found in the following document: Oddy Test Methods Chart.

Current Version: 20171116_OT
22 March 2018
Buscarino, I. C., Stephens, C. H., and Breitung, E. M.

This method adopts aspects from the protocol published by The British Museum[1], where test tubes are fitted with silicone stoppers holding three metal coupons, and the Met’s original three in one jar version [2], where metals are hung from the rim of a beaker inside of a screw-top jar. In both cases, the corrosion states of the coupons after 28 days of aging at elevated temperatures and humidity in the presence of an unknown material are used to determine the appropriateness of a material for use in close proximity to cultural heritage materials.

The Met’s previous version (20160416_OT), which is downloadable from the AIC’s Oddy test wiki site, incorporated silicone stoppers pressed into the neck of screw-top Pyrex™ jars. We observed significant inconsistencies in stopper quality and production time, which lead us to identify replacement options. The current version (20171116_OT), which is downloadable from the AIC’s Oddy test wiki site, replaces the silicone stoppers and o-rings with Viton™ o-rings and 3D printed nylon ‘hangers’ that fit into the neck of screw-top Pyrex™ jars. We have had much greater success with repeatability of controls with method 20171116_OT than previous methods.
This document includes written instructions and links to video demonstrations of the method. Each change has been labeled as a new version of the test using the following format YEARMODA_OT indicating the year (YEAR), month (MO), and date (DA) the modification was implemented. A list of versions will be added to this document in the near future to correlate to results being published on the AIC Oddy Test wiki site.

  1. Korenberg, C., Keable, M., Phippard, J., Doyle, A. “Refinents Introduced in the Oddy Test Methodology”, Studies in Conservation, (August 2017), online article, 1-12.
  2. Bamberger, J. A., Howe, E. G., Wheeler, G., A Variant Oddy Test Procedure for Evaluating Materials Used in Storage and Display Cases, Studies in Conservation 44 (1999) 86-90.

Outline:
I. Personal Protection Equipment (PPE)
II. Washing Methods
III. Metal Coupon Preparation
IV. Jar preparation and assembly
V. Assessment at completion of testing
VI. Photographing Oddy Test Coupons
VII. Materials and Supplies
VIII. Oddy Test Material Sample Preparation Guide
IX. Oddy Test Form


I. Personal Protection Equipment (PPE): Nitrile gloves, safety glasses, and a laboratory coat are worn throughout this procedure. Hands are washed with soap and warm water prior to donning gloves to remove oils. Care is taken to always handle the metal coupons (copper [Cu], lead [Pb], or silver [Ag]) with tweezers while wearing clean nitrile gloves, as handling coupons with dirty or oily hands can cause coupon contamination. Out of a small range of gloves, Freeform® SE blue powder-free nitrile gloves performed best in the Met’s Oddy test and are worn throughout the procedure.

II. Washing Methods: Outlined below are two different washing methods. The hand washing method was used April 2016 to July 2017. The dishwasher method began in July 2017 and is our current washing method.

A) Dishwasher Method Used June 6, 2017-current (method 20170606_OT)
Using Lancer 815 LX Dishwasher
Glassware: Mechanically remove all materials from jar. Place each jar over a spindle jet. The wash cycle includes the following steps:
Prewash Rinse for 2 min.* with 60°C water
Wash (base) Rinse with 96 mL of NaOH in 12 L of water at 40°C for 2 min.*
Rinse A Rinse for 2 min. with unheated water.
Acid Rinse Rinse with 96 mL of Phosphoric Acid in 12 L of unheated water for 2 min.
Rinse B Rinse for 3 min. with unheated water.
Rinse C Rinse for 3 min. with unheated water.
Purified Water Rinse A Rinse for 3 min. with unheated 15 MΩ-deionized water.
Purified Water Rinse B Rinse for 1 min.* with 60°C 15 MΩ-deionized water.
*When water is being heated, it is recycled within the chamber until it reaches temperature making the times listed much shorter than the actual cycle time. After the washer reaches the prescribed temperature, it runs for the programmed amount of time. The full wash cycle requires approximately 1.75 hours. Detergents are not currently used, however, testing is underway to determine if their use improves consistency of results.

Washed glassware placed in a 60°C oven for drying and storage.
O-ring, lids, and silicone stoppers: Place on flat stainless steel mesh rack. Lids are placed upright and are weighted with a stainless steel mesh screen to inhibit flipping. The wash cycle includes the following steps:
Prewash Rinse for 2 min.* with 80°C water
Rinse A Rinse for 5 min. with unheated water.
Rinse B Rinse for 1 min.* with 80°C water.
Purified Water Rinse A Rinse for 1 min. with unheated 15 MΩ-deionized water.
Purified Water Rinse B Rinse for 1 min.* with 60°C 15 MΩ-deionized water.
*When water is being heated, it is recycled within the chamber until it reaches temperature making the times listed much shorter than the actual cycle time. After the washer reaches the prescribed temperature, it runs for the programmed amount of time. The full wash cycle requires approximately 2.5 hours. Detergents are not currently used, however, testing is underway to determine if their use improves consistency of results.

Washed o-rings, lids, and silicone stoppers are dried and stored in a 60°C oven.
Vials: KIMAX™ vials are washed by hand.
  1. Dirty vials are placed in a 50 mL Pyrex® beaker, and a disposable glass pipet is used to deliver solutions into the vials. Soak vials with Micro 90 Lab cleaner for at least 24 hours (1% solution in tap water). Rinse 3 times with tap water. Soak in room temperature aqueous sodium hydroxide (NaOH) bath with a pH of 12 for at least 15 hours (overnight). Use 10” stainless steel tongs for delivering and retrieving items from the baths. Thick nitrile gloves, safety glasses, and a laboratory coat are required.
    a. Base bath preparation (yields 1 L): Add 0.40 g NaOH (s) to 1 L of deionized H2O. Check that the pH reads 12 on the pH indicator strip. The base bath is in a glass beaker contained in a lidded polypropylene 12 quart container within a secondary polypropylene drip container.
  2. Rinse with hot tap water then place in a hydrochloric acid (HCl) bath with a pH of 2 for at least 15 hours (overnight). Thick nitrile gloves, safety glasses, and a laboratory coat are required.
    a. Acid bath preparation (yields 1 L): Slowly add 0.8 mL HCl (37% w/w; 1.2 g/mL density) to 250 mL of deionized H2O. Add the remaining 750 mL of deionized H2O. Check that the pH reads 2 on the pH indicator strip. The acid bath is in a glass beaker contained in a lidded polypropylene 12 quart container within a secondary polypropylene drip container.

Base acid baths.PNG
Figure 1: Base and acid baths in secondary containers.

  1. b. Rinse three times with hot tap water then rinse three times with 18.2 mΩ-deionized water.
    c. Dry in an oven, right side up, at 60°C.

B) Hand-washing Method Used April 2016-May 2017 (method 20160416_OT)
Glassware Preparation:
  1. Wash with Micro-90 Lab Cleaner (1% solution in tap water) using a laboratory cleaning brush and tap water.
  2. Rinse 3 times with hot tap water.
  3. Soak in room temperature aqueous sodium hydroxide (NaOH) bath with a pH of 12 for at least 15 hours (overnight). Use pipets to deliver the solutions into the small vials. Use 10” stainless steel tongs for delivering and retrieving items from the baths. Thick nitrile gloves, safety glasses, and a laboratory coat are required.
    a. Base bath preparation (yields 7 L): Add 3.0 g NaOH (s) to 7.5 L of deionized H2O. Check that the pH reads 12 on the pH indicator strip. The base bath is contained in a lidded polypropylene 12 quart container within a secondary polypropylene drip container.
  4. Rinse with hot tap water then placed in a hydrochloric acid (HCl) bath with a pH of 2 for at least 15 hours (overnight). Thick nitrile gloves, safety glasses, and a laboratory coat are required.
    a. Acid bath preparation (yields 7 L): Slowly add ~6 mL HCl (37% w/w; 1.2 g/mL density) to 2 L of deionized H2O. Add the remaining 5 L of deionized H2O. Check that the pH reads 2 on the pH indicator strip. The acid bath is contained in a lidded polypropylene 12 quart container within a secondary polypropylene drip container.
  5. Rinse three times with hot tap water then rinse three times with 18.2 mΩ-deionized water.
  6. Dry in an oven, right side up, at 60°C.

Viton™ o-rings and lids:
  1. Wash lids and Viton™ o-rings in a Micro-90 Lab Cleaner solution (1% in tap water) by dipping in cleaning solution and rubbing with gloved hands or a clean sponge. Do NOT soak for any length of time in Micro-90 Lab Cleaner solution.
  2. Rinse 3 times with hot tap water and 3 times with 18.2 MΩ-deionized water.
  3. Store in oven at 60°C.

KIMAX™ Vials: Same as instructions outlined in the dishwashing method section II-A above.

III. Metal Coupon Preparation

  1. Measure and cut high purity (99.998% or higher) metals (Ag and Cu) into coupons measuring 0.8 cm x 2.5 cm.
    a. Use a dedicated pair of scissors for each metal.
  2. Place a 12” x 12” flat glass plate on the counter. Sand both sides of the lead coupon (Click here for video), sanding only along the length of the coupon, away from the user, using an unused area of folded 3200 grit Micromesh™ sand paper using even, light pressure. Each side of the long strip of lead should take approximately 35 seconds to sand. Anything longer tends to result in over-sanding. Consistent sanding is critical for producing reproducible test coupons. The idea is to remove the native oxide with minimal pressure. Printing and hanging enlarged images of over-sanded and correctly sanded lead coupons in the preparation area is recommended for reference. See Figure 2 below for an example of properly sanded lead and shiny over-sanded lead. The sanding process is completed in a hood with ULPA filtration (Click here for video).
    a. Sand lead coupons immediately before inserting into jars to minimize re-oxidation of the surface.

Lead sanding.PNG
Figure 2: Left: a properly sanded lead coupon. Middle: a partially over-sanded lead coupon. Right: a fully over-sanded shiny lead coupon.

  1. Soak copper and silver coupons in a small beaker of acetone and wipe dry with a Kimwipe®. Next, soak the coupons in fresh HPLC grade isopropanol. Remove from beaker and wipe dry with a Kimwipe® (Click here for video). Collect rinse solutions and disposed of as hazardous waste.
  2. After sanding 0.8 cm x 10 cm lead strips, rinse each side with acetone from a wash bottle and gently wipe with a Kimwipe®. Repeat. Next dip a Kimwipe® in isopropanol and wipe each side of the lead strip. Repeat. (Click here for video). Cut each lead strip into four 0.8 cm x 2.5 cm coupons.

Unaged coupons.PNG
Figure 3: Freshly cut and sanded (lead only) metal coupons.

  1. After polishing and rinsing, dispose of Mylar™, Pb-contaminated gloves, and sandpaper as lead-contaminated hazardous waste.
  2. All metals are stored immediately upon receipt from the supplier in at least one Intercept® Ziploc®-style bag. Ideally both sides of the bag are composed of the Intercept material rather than using the style with a transparent window.

IV. Jar preparation and assembly

  1. Run all tests in duplicate, including controls. Produce one set of controls for each group of tests. In other words, if 15 materials are being tested on Monday, one set of controls is required. A new set of controls is required for the next group of Oddy tests that are prepared on Tuesday.
  2. To prepare one jar, place a sheet of weighing paper on the scale and tare to zero. Weigh 2g of test sample material on the paper and load into a 100 mL borosilicate jar (Kimble™ KIMAX™ GL 45 Media/Storage Bottles, Product # 02-542A, 100mL) along with a borosilicate mini-test tube (Kimble™ KIMAX™ Reusable Borosilicate Glass Tubes with Plain End, Product #14-925B, 0.7mL) containing 0.5mL 18.2 MΩ-deionized water. Dose 18.2 MΩ water into the mini-test tube using a recently calibrated micropipette.
    a. See Section VIII for a sample preparation guide.
    b. Each control jar contains 0.5 mL of water in the KIMAX™ test tube as well as the metal coupons inserted into a stopper. No other material is placed in the jar.
  3. To a pre-washed new 3D printed nylon coupon holder, attach the metal coupons by bending the coupon 5-7mm from one end and crimping it onto the holder (see Figure 4). Insert the coupon holder into the mouth of the jar.
    a. Make sure coupons do not contact each other, the jar, or test material.

Nylon holders.PNG
Figure 4: the triangle-configured 3D printed nylon holder ordered from Shapeways.

Holders with coupons.PNG
Figure 5: Left: crimping the Cup coupon onto the holder using tweezers. Right: A coupon holder with Cu, Ag, and Pb coupons attached.

Jars with sample.PNG
Figure 6: Left: a coupon holder placed in the neck of a sample jar. Center and Right: A sealed sample jar with hanger, coupons, test material, water and vial.

  1. Weigh jars and record values.
  2. Place in oven leaving as much space between jars as possible for air circulation, standing upright.

Torque wrench.PNG
Figure 7 & 8: Custom torque wrench socket produced to fit GL45 cap and CDI 1502MRMH-QR torque wrench (2.8-16.4 Nm range) used for tightening lids consistently.

  1. Leave jars in oven at 60°C for 60 minutes. Remove jars and re-tighten lids to a torque of 4 Nm while warm using a torque wrench fitted with the custom socket.
  2. Return jars to the oven and age at 60 ± 1.5 °C for 28 days.


V. Assessment at completion of testing

  1. After 28 days in the oven, remove jars and allow to cool to room temperature.
  2. Record weights of each jar. Compare to the pre-aged weights to determine whether each vessel was sealed during the experiment. A loss greater than 25% of mass (25% of 0.5 grams, or a loss of more than 0.13 grams) is considered a system failure, and the experiment is repeated.
  3. Open jars and lift the coupon holders out of the jars. Remove coupons from the coupon holders using tweezers.
  4. Unfold the coupon where it was crimped over the coupon holder. Scribe the inside of each coupon across the width of the coupon where it met with the holder using a dissection needle. Press the coupons flat using two blocks of polished flat stainless steel, aluminum, or glass. Place the coupons on a fresh piece of aluminum foil or petri dish.
  5. Inscribe the letter “C” in the portion of the control coupons that were inserted into the stopper. Assess the controls for corrosion. If they are minimally corroded, proceed. If the coupon corrosion of a given metal in one jar is significantly different from that in the other or if there is significant corrosion, repeat the experiment.
  6. Using a spatula, remove the o-ring from the lid. Save and wash o-rings from “permanent” test jars. Consider sorting and saving ‘Temporary’ o-rings. Also consider sorting out ‘Unsuitable’ lids. It may be that with proper treatment, they can be safely reused. The Met is currently not reusing temporary or unsuitable o-rings, and not reusing unsuitable lids.

Lead

Lead control.PNG
Figure 9 & 10: Left: acceptable amount\ of minimal corrosion for control. Right: too much corrosion, observed as darkening, for control.

Copper

Copper control.PNG
Figure 11 & 12: Left: acceptable amount of minimal corrosion for control. Right: too much corrosion, observed as reddening, for control.

Silver

Silver control.PNG
Figure 13 & 14: Left: acceptable amount of minimal corrosion for control. Right: too much corrosion, observed as yellowing, for control. Note: silver control coupons rarely show corrosion.

  1. The following ratings are used to assess non-control coupons:
a. “Permanent” rating: The material tested may be used indefinitely in the presence of art.
i. Coupons look similar to the controls.
ii. Silver: remnants of polishing compounds from some manufacturers can develop or appear as white splotches. This stock is generally returned to the manufacturer, however, if it makes it into a test, the white splotches are ignored.
b. “Temporary” rating: The material is safe for use near but not in contact with art for up to six months.
i. Copper: slight reddening, yellowing, or rainbow-like color change, formation of up to 20 black spots
ii. Silver: slight yellowing, purpling, or darkening.
iii. Lead: darkening, yellow/olive tarnish, haze from slight crystal formation over the entire coupon, or heavier crystal formation at the interface with the coupon holder.
c. “Unsuitable” rating: the material should not be used in contact with or near art and another material should be found.
i. Copper: severe blackening or severe reddening or matte-textured surface.
ii. Silver: severe color change to dark purple, yellow, or black.
iii. Lead: white fluffy crystal formation.

Photos of scored coupons from permanent, temporary, and unsuitable categories can be downloaded from the links listed at the top of this protocol.


"'VI. Photographing Oddy Test Coupons'"
After being evaluated, Oddy test coupons with matching duplicate results and passing control jars are photographed using two different types of lighting: diffuse lighting using a Rosco LitePad HO90 12”x12” (figure 17), and glancing-angle lighting using a Cree XLamp CXA3050 LED with a Mean Well HLG-100H-36A power supply (figure 18). The diffuse lighting allows for proper color representation in the photograph. Glancing-angle lighting allows for the representation of surface texture in the photograph. Coupons are placed on an angled stage in between the Rosco LitePad and the white piece of paper board used to diffuse light. A photograph is taken using the diffuse lighting and another one is taken using the glancing-angle lighting. Photographs are color-corrected and processed in Lightroom.
Photo set up.PNG

Diffuse light set up.PNG


Glancing angle light set.PNG


VII. Materials and Supplies

Metal Preparation Material

'Photographing Equipment

VII. Oddy Test Material Sample Preparation Guide

Material Proposed Cutting Method
Board - composite (eg. Corian, drywall) Cut with universal blade band saw into 0.5” cubes. Use utility knife to produce smaller pieces to make 2.0g.
Board - natural (eg. wood, cotton) Cut with universal blade band saw into 0.5” cubes. Use utility knife to produce smaller pieces to make 2.0g.
Board - plastic/polymeric/synthetic Cut with universal blade band saw into 0.5” cubes. Use utility knife to produce smaller pieces to make 2.0g.
Carpet - natural/non-syntheticfiber Cut with scissors or utility knife into 1 x 1” squares. To reach 2.0 g, cut pieces that represent the sample’s composition—example: the correct ratio of carpet material, blended fibers in carpet, and base of carpet.
Carpet - plastic/polymeric/synthetic fiber Cut with clean scissors or utility knife into 1 x 1” squares. To reach 2.0 g, cut pieces that represent the sample’s composition—example: the correct ratio of carpet material, blended fibers in carpet, and base of carpet.
Coating - floor (e.g. stain, anti-wear, anti-slip) Follow manufacturer’s instructions regarding dilution; if to be used dry, paint out on Mylar® and cure per manufacturer’s guidelines; if to be used wet, use 0.5mL of liquid in lieu of water.
Coating - grease, oil, wax Into a 5mL beaker, weigh 2.0 g of sample. Carefully place into the sample jar. Other borosilicate vessels that fit are acceptable as long as they are no more than 4cm tall.
Coating - paint & primer Paint material onto a Mylar® sheet and spread to a thickness that reflects how it will be used in the museum. Cure the material according to manufacturer’s instructions. After curing, cut the painted Mylar® into 1.5” wide strips and weigh to 2.0 g, taking the weight of the Mylar® into account by subtracting it from the total sample weight. Put a small piece of Mylar® at the bottom of the jar if there’s concern about the material sticking to the glass. Roll the sample strips into a coil with the sample material facing inward, and place in the bottom of the jar.
Coating - protective (e.g. anti-UV, -abrasion, -tarnish) Paint the material onto a Mylar® sheet and spread to a thickness that reflects how it will be used in the museum. Cure the material according to manufacturer’s instructions. After curing, cut the painted Mylar® into 1.5” wide strips and weigh to 2.0 g, taking the weight of the Mylar® into account by subtracting it from the total sample weight. Put a small piece of Mylar® at the bottom of the jar if there’s concern about the material sticking to the glass. Roll the sample strips into a coil with the sample material facing inward, and place in the bottom of the jar.
Fabric - batting & padding Cut material with clean fabric scissors into 1 x 1” squares. To reach 2.0 g, cut small segments from a 1” square.
Fabric - book cloth Cut material with clean fabric scissors into 1 x 1” squares. To reach 2.0 g, cut small segments from a 1” square.
Fabric - exhibition/woven Cut material with fabric scissors into 1 x 1” squares. To reach 2.0 g, cut small segments from a 1” square.
Fiber or Thread Cut the length of sample that weighs 2.0 g. Wind it loosely and neatly around two gloved fingers, remove, and place in the bottom of the sample jar.
Inorganic - (e.g. fillers, salts, rocks) Keep the sample as is or prepare it as it would be used in the museum. For example, if you are testing salts, do not grind them further unless that’s how they are used in the museum setting. Weight 2.0 g of sample.
Metal - mechanical fastener Place whole fastener in jar.
Paper-based (e.g. folder, cardboard, sheet) Cut material with clean scissors into 1 x 1” squares. To reach 2.0 g, cut pieces from a 1” square.
Paper-based, Filled (e.g. fillers such as silica gel, zeolites, alumina) Cut material with clean scissors into 1 x 1” squares. To reach 2.0 g, cut pieces from a 1” square.
Paste - filler/binder mixture (e.g. plaster, acrylic spackle, non-paint) Extrude onto a Mylar® sheet. Spread to a thickness that reflects how it will be used in the museum setting. Cure material per manufacturer’s suggestion. After cured, peel the material from the Mylar® if possible and weigh to 2.0 g. If the material cannot be freed from the Mylar®, remove excess Mylar® and weigh the material to 2.00 g, taking the weight of the Mylar® into account by subtracting it from the total sample weight.
Polymer - adhesive - caulk or sealant Extrude onto a Mylar® sheet. Spread a thickness that reflects how it will be used in the museum setting. Cure per manufacturer’s instructions. After curing, peel the material from the Mylar® if possible and weigh to 2.0 g. If the material cannot be freed from the Mylar®, remove excess Mylar® and weigh the material to 2.0 g, taking the weight of the Mylar® into account by subtracting it from the total sample weight.
Polymer - adhesive - glues - liquid (e.g. acrylics, wood glues, starches) Extrude adhesives onto Mylar® sheeting in a thickness that reflects the actual material application thickness. Cure per manufacturer’s instructions. Cut the sample into 1 x 1” squares. Weigh the dried material on Mylar®, taking into account the weight of the Mylar® attached to the sample. To reach 2.0 g, cut pieces from a 1 x 1” square.
Polymer - adhesive - heat activated (e.g. hot melt, heat set) Extrude 2” strips of melted material onto aluminum foil. Allow to cool. Peel from aluminum foil and weigh out 2.0 g of sample. If material does not remove from foil, repeat on Mylar® and account for the weight of the Mylar® in weighing the sample.
Polymer - adhesive - pressure-sensitive Cut 2” lengths of tape, taping the adhesive sides, to the backed sides to form a small 2.0 g block of tape. Place the sample onto Mylar® to protect the jar from the adhesive
Polymer - adhesive tape - double sided Fold the tape onto itself “accordion style” every 2” while removing the backing. Put 2.00 g sample on a piece of Mylar® to protect the jar from the adhesive, and carefully place in the bottom of the jar.
Polymer - adhesive tape - single sided Cut 2” lengths of tape, taping the adhesive sides, to the backed sides to produce a small 2.0 g block of tape. Place the sample onto Mylar® to protect the jar from the adhesive
Polymer - block/bulk/pellet If material comes in a block, cut into 0.5” cubes using a band-saw. If the material comes in small pellets that fit in the sample jar, use whole uncut pellets. To reach 2.0 g, shave material from one cube or pellet using a utility knife.
Polymer - foam - building insulation For dense foam, cut with universal band saw into 0.5” cubes. To reach 2.0 g, remove material from one cube using a utility knife.

For soft foams, cut material with clean scissors into a 1.5” wide strip that weighs 2.0 g. Compress the strip into a roll, and insert into the bottom of the jar. Make sure the foam does NOT touch the metal coupons when it expands.

Polymer - foam - non building insulation For dense foam, cut with universal band saw into 0.5” cubes. To reach 2.0 g, shave any excess material on only one cube using a utility knife.

For soft foams, cut material with scissors into a 1.5” wide strip that weighs 2.00 g. Compress the strip into a roll, and insert into the bottom of the jar. Make sure the foam does NOT touch the metal coupons when it expands.

Polymer - foam sealant Cut material with clean scissors into a 1.5” wide strip that weighs 2.0 g. Compress the strip into a roll, and insert into the bottom of the jar. Make sure the foam does NOT touch the metal coupons when it expands.
Polymer - gasket Cut material with clean scissors into 2” length strips.
Polymer - glove Cut material with clean scissors into 1 x 1” squares. To reach 2.0 g, cut pieces from a 1” square.
Polymer - membrane (<1mm thick) Cut material with clean scissors into 1 x 1” squares. To reach 2.0 g, cut pieces from a 1” square.
Polymer - sheet (>1mm thick) Cut material with clean scissors into 1 x 1” squares. To reach 2.0 g, cut a minimal amount of strips from a 1” square.



Indianapolis Museum of Art at Newfields (IMA) Protocol

Oddy test procedure:

All Oddy tests were performed using the modified British Museum 3-in1 procedure. In this test, a 2g sample of the material to be studied is placed in a borosilicate boiling tube with a small vial containing 0.8mL of deionized water. Freshly polished copper (Aldrich, 0.25mm, 99.98%), silver (Aldrich, 0.25mm, 99.9%), and lead (Alfa Aesar, 0.1mm, 99.998%) coupons are fixed into a silicone stopper, and the stopper is sealed onto the test tube using Parafilm and PTFE tape. Each sample and a control with no sample are studied in triplicate. The tubes are placed upright in a rack in a thermostated oven at 60°C for 28 days.

Cleaning of glassware:
• Glassware is cleaned with water and detergent following each run.
• Washed with sink water, then rinsed with distilled, and reverse osmosis water.
Set Up:

IMA Oddy Test SetUp





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